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Ice Crystallization
in Ice Cream
Production
K.L.K. Cook and R.W. Hartel
ABSTRACT: The smoothness and perceived quality of an ice cream depends in large part on the small size of ice
crystals in the product. Understanding the mechanisms responsible for producing the disc-shaped crystals found
in ice cream will greatly aid manufacturers in predicting how processing and formulation changes will affect their
product. Because ice cream mix is opaque, it has not yet been possible to observe ice crystallization in ice cream in
situ. Studies to date, therefore, have used analogues or have related observed effects to a hypothesized mechanism.
Still, some elements of the crystallization mechanism are well accepted. Because of the large supercooling at the
freezer wall, ice nucleates there before being swept into the bulk of the freezer. In the bulk, heat and mass transfer
cause some crystals to melt and others to grow. By the time the ice cream reaches the freezer exit, the ice crystals
have become small, rounded discs.
Introduction
The delights of ice cream have been known in the western
world since Marco Polo returned from Far East Asia in the 13th
century bringing with him recipes for water ices. Over time, these
water ices evolved into the popular frozen desserts of today. Modern ice cream is a partially-frozen mixture of milk, cream, sugar,
stabilizers, and emulsifiers. Its apparent simplicity belies the complicated structure inside Americas favorite frozen treat. Ice cream
is equally an emulsion, a dispersion, and a foam. The dispersion
and emulsion consist primarily of a freeze-concentrated aqueous serum phase containing sugar and the dry matter contents
surrounding dispersed ice crystals and fat globules (Marshall and
others 2003). Ice crystals range in size from about 1 to over
150 m in diameter, with an average size of about 35 m (Berger
and others 1972; Caldwell and others 1992; Donhowe and Hartel 1996a; Hagiwara and Hartel 1996; Hartel 1996; Koxholt and
others 2000; Marshall and others 2003; Sofjan and Hartel 2004;
Inoue and others 2008; Kusumaatmaja 2009). Fat globules are 2
m or less in diameter (Marshall and others 2003). The foam is
formed by pockets of air (about 20 to 50 m diameter) dispersed
throughout the emulsion and is supported by partially-coalesced
fat globules (Goff 2002; Marshall and others 2003).
The best ice creams on the market have a smooth and creamy
texture. That creamy texture, primarily associated with a high fat
content, is also determined, in part, by the average size of the
ice crystals. Larger crystals (greater than 50 m) impart a grainy
MS 20090967 Submitted 9/30/2009, Accepted 10/25/2009 . Authors are with
Univ. of Wisconsin Madison, 1605 Linden Dr., Madison, WI 53706, U.S.A.
Direct inquiries to author Hartel (E-mail: rwhartel@wisc.edu).
c
R
2010 Institute of Food Technologists
213
2 T
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(1)
Nucleation is the birth of a crystal (Hartel 2001). In a scrapedsurface freezer, this only occurs at the wall of the freezer where
the temperature gradient is high enough to form new crystals.
The rate of nucleation is important because it affects the number
of crystals in a product, which in turn affects how large each
crystal can become. For ice cream, once it exits the freezer, the
maximum number of ice crystals is set, and those crystals continue to grow until the amount of ice is in equilibrium with the
temperature (Hartel 1996).
The nucleation process starts with the initial cluster of ice as a
loose aggregation of molecules. As the cluster loses energy, the
molecules become more ordered and a lattice structure begins
to form and the cluster becomes an embryo. When the embryo
grows large enough to be in thermodynamic equilibrium with the
solution and when the embryo overcomes the energy barrier to
nucleation, it is a nucleusthe smallest collection of molecules
in a crystal lattice that will not redissolve. When the nucleus
grows it becomes a crystal (McCabe and others 2005).
Nucleation can occur in several ways. Primary nucleation describes the spontaneous formation of a nucleus from solution,
whereas secondary nucleation describes the formation of a nucleus from a preexisting crystal or crystal fragment. There are 2
types of primary nucleation: homogeneous and heterogeneous.
In homogeneous nucleation, the nucleus is formed in the bulk
of the fluid by molecular accretion (McCabe and others 2005).
In heterogeneous nucleation, on the other hand, the nucleus
forms on a foreign particle or object, which could be anything
from a dust mote to the wall of an ice cream freezer (Hartel
2001). Because heterogeneous nucleation occurs more readily
and with less supercooling than does homogeneous nucleation,
it is much more common in practical applications (Schwartzberg
1990). Secondary nucleation most commonly occurs in industry as contact nucleation, which is when a crystal collides with
another crystal, the wall, or an agitator (McCabe and others
2005).
Several factors affect nucleation. The most important factor is
the driving forcethe temperature difference between the solution and its freezing point. A greater driving force increases nucleation. However, when the temperature is too low, decreased
molecular mobility slows nucleation. Below the glass transition
temperature, T g , no nucleation occurs. Agitation can enhance nucleation in a labile (ready-to-nucleate) system. Cooling rate influences nucleation as well. For example, if no nucleation is desired,
the solution can be quickly cooled to a temperature below the
glass transition before the onset of crystallization (Hartel 2001).
In foods, the formulation and ingredients can impact nucleation;
for instance, sucrose may slow ice nucleation (Schwartzberg
1990).
Growth
215
(2)
(3)
Figure 2 --- Three-dimensional schematic diagram of ice crystallization and fluid flows through a scraped-surface heat
exchanger for ice cream manufacture. The scraper blade removes a slush of ice crystals and concentrated ice cream
mix from the barrel wall in flocs, the dasher breaks apart these ice flocs, and the warm bulk liquid melts the flocs
apart into disc-shaped crystals. Near the inlet, the warm bulk temperatures melt the majority of the ice. As freezing
continues more ice crystals survive in the bulk. Close to the exit, the bulk crystals are larger; the wide size range
causes many small new crystals to melt.
the center (Hartel 1996). Axially, from the inlet to the outlet along
the barrel center, the temperature has been shown to decrease
rapidly in the first 15% of the barrel to between 3 and 7 C
and then decrease linearly to just before the freezer exit, where
the temperature increases by about 1 C (Hartel 1996; Russell
and others 1999).
Initial freezing is a dynamic process: the mix is frozen while
being agitated, which whips in the air, destabilizes the fat, and
scrapes ice into the bulk fluid (Goff 1997; Marshall and others
2003). As illustrated in Figure 2, cold ice cream mix enters the
freezer, with the refrigerant absorbing the heat in the mix until
the supercooling at the wall is great enough to initiate ice nucleation. As ice crystals form at the wall, the dasher blades scrape
the surface layer from the wall about every 0.075 s, assuming 4
blades with a dasher speed of 200 rpm, and propel the ice layer, at
a temperature of 20 to 25 C (Hartel 1996), into the bulk of the
freezing ice cream mix. This is pictured schematically in Figure 2,
with a larger, cross-sectional view shown in Figure 3. In the bulk,
the warmer temperatures cause the ice crystals to ripen into disclike shapes. The details on how the ice crystals actually form
and ripen is still the subject of research, although several theories
have been proposed (see next section). When the ice cream exits the freezer, it is usually around 5 to 6 C, and close to
half of the water is frozen. From a survey of recent studies, the
average ice crystal size exiting an ice cream freezer is 20 to 30
m (Donhowe and Hartel 1996a; Hartel 1996; Russell and others 1999; Chang 2000; Windhab and Wildmoser 2002; Marshall
and others 2003; Sofjan and Hartel 2004; Drewett and Hartel
2007).
Based on the axial temperature profile in a SSF, ice cream
freezing generally follows the solid-liquid equilibrium curve on
an ice cream mix phase diagram. Figure 4 shows an approximate phase diagram for ice cream mix. The actual freezing point
for an ice cream mix can be calculated from published equations (Bradley 1984; Marshall and others 2003) and is based
on the type and content of sweeteners and other solids in the
mix. As freezing begins, the ice crystals formed are purely frozen
water (Omran and King 1974), which leaves the solutes dissolved
in less water than before. As freezing continues and the serum
phase is further concentrated, the freezing point decreases until
the target temperature has been achieved. If the ice cream is fur-
217
Figure 4 --- Sample phase diagram for ice cream mix containing 10% milk solids nonfat, 16% sucrose, and 38%
total solids; Tg is the glass transition temperature at
is the end of the freezmaximal freeze concentration, Tm
ing point curve, and Cg is the maximal freeze concentration (Hartel 1996; Marshall and others 2003; Schawe
2006). The dashed lines indicate that there is a degree
of uncertainty when predicting the glass transition curve
and the freezing curve for ice cream mix with high solids.
Freezing Mechanisms
The specific mechanisms of ice crystal formation in a scrapedsurface heat exchanger during ice cream manufacture remain
somewhat elusive. No one has yet been able to observe ice crystals forming while making ice cream, mainly because ice cream
mix is opaque and the freezer barrel is enclosed. Various studies, therefore, have resorted to either using sucrose solutions as
model systems for ice cream (Omran and King 1974; Stocking
and King 1976; Schwartzberg and Liu 1990; Sodawala and Garside 1997; Jacobsen 1999; Si 2000; Lian and others 2006; Zheng
2006) or to examining cause-and-effect relationships when
making ice cream in an SSF (Cebula and Russell 1998; Russell
and others 1999; Drewett and Hartel 2007).
Crystal morphology is of fundamental importance to describing
how ice forms in an SSF. If the crystals are initially disc-shaped,
they will ripen differently than if the ice leaves the freezer wall
in dendritic form. Numerous studies have attempted to define
the initial ice crystal shape formed in an SSF. In freezing sugar
solutions, disc-shaped crystal morphologies were observed at
very low supercooling (under 100 mK). At higher supercoolings,
such as in an SSF, however, dendritic or needle-like morphologies occurred (Stocking and King 1976). In quiescently-frozen
sugar solutions, as well, dendritic growth is well-known to occur
(Macklin and Ryan 1966; Omran and King 1974). At constant
supercooling, increasing the sugar concentration delays nucleation and causes crystal size to decrease (Omran and King 1974;
Schwartzberg 1990). For dendrites, increasing sugar content also
causes thinner branches (Schwartzberg 1990).
Based on the principles of dendrite formation, Schwartzberg
proposed the lawnmower model. Schwartzbergs experiments
involved observation of sucrose solution quiescently-frozen on a
chilled surface (Schwartzberg and Liu 1990). Because the experiments used quiescent freezing, dendritic growth was observed.
However, he suggested that due to the high supercooling at the
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Conclusions
The final structure and sensory properties of ice cream are a
function of many different processing and formulation variables
that tend to be a complex function of one another. Ice cream companies today already are able to produce high-quality ice cream.
However, with the ongoing quest to make products healthier,
longer-lasting, cheaper, and/or of higher quality, understanding
the effects of the numerous variables and their interactions helps
both scientists and engineers. This understanding allows scientists to better predict the effects of processing and formulation
changes and allows engineers to optimize plans and to make
improved assumptions in models.
Existing research has made great strides in elucidating the
mechanisms of ice crystallization in the ice cream freezer, though
more research is still needed to obtain the definitive model. The
vast majority of research has looked at ice crystallization in model
solutions in model systems. Ideally, scientists will one day be able
to piece together how ice forms in ice cream mix in its actual system.
Nomenclature
Roman letters
C = Concentration, g solute/g solution; C g , maximum
freeze concentration
n = Variable parameter, dimensionless
r = Radius, m; r, average radius; r0 , initial average
radius
R = Recrystallization rate, m/s1/n
t = Time, s
T = Temperature, K; T g , glass transition temperature;
T g , glass transition temperature at maximum
freeze concentration; T m , onset of melting at
maximum freeze concentration; T ,
temperature at infinite radius
Greek letters
H fus = Latent heat of crystallization, J/kg
T = Freezing point depression, K
s = Crystal density, kg/m3
= Interfacial tension (surface free energy per unit
area), J/m2 or N/m
= Variable parameter, s/mn
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